Assessment of Major and Minor Metals Levels in Selected Libyan Palm Dates Fruits

Abstract

In the current study, five Dates cultivars from Misurata City in Libya were collected during the harvest season. These cultivars were: al-Tabouni (TAB), al-Bakrari (BAK), al-Aami (AAM), al-Hamouri (HAM), and al-daqla (DAQ). The samples were analyzed for their moisture, ash, and metals contents. Flame photometry was used to determine K, Mg, Na, and Ca. The other elements (Fe, Zn, Cu, Cd, and Pb) were determined via flame atomic absorption spectrometry. The metal concentrations range in dry weight were as follows (mg/kg): K (

Full text

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Journal of Applied Science and Environmental Studies
JASES
http://revues.imist.ma/index.php?journal=jases
Original Paper
ASSESSMENT OF MAJOR AND MINOR METALS LEVELS IN
SELECTED LIBYAN PALM DATES FRUITS
K. M. ELSHERIF1, A. M. ALJAROUSHI2
1Chemistry Department, Faculty of Science, University of Benghazi, Benghazi, Libya
2Department of Nutrition, Faculty of Medical Technology, Misurata, Libya
Received 24 August 2021; Revised 28 September 2021, Accepted 20 October 2021.
Keywords
Phoenix dactylifera L
Palm Date
Essential metals
Heavy metals
Abstract
In the current study, five Dates cultivars from Misurata City in Libya
were collected during the harvest season. These cultivars were: al-
Tabouni (TAB), al-Bakrari (BAK), al-Aami (AAM), al-Hamouri
(HAM), and al-daqla (DAQ). The samples were analyzed for their
moisture, ash, and metals contents. Flame photometry was used to
determine K, Mg, Na, and Ca. The other elements (Fe, Zn, Cu, Cd, and
Pb) were determined via flame atomic absorption spectrometry. The
metal concentrations range in dry weight were as follows (mg/kg): K
(2146.1- 3393), Mg (69.0- 167.1), Ca (24.0-64.0), Na (17.0-69.0), Fe
(8.4-127.9), Zn (4.95-12.13), Cu (3.12-5.27), Cd (0.00-0.58), and Pb
(0.00-0.64). The predominant macro mineral was potassium, and the
main heavy metal was iron. Considering the nutrition value, dates are
an important product since they are a good source of essential minerals.
Two date cultivars, DAQ and BAK; showed the presence of significant
amounts of the Pb and Cd. The levels of Cd and Pb in the fruit tissue
are increased with increasing anthropogenic sources. Consequently,
date palm fruits might be utilized as a pollution indicator.
1. Introduction
One of the oldest cultivated trees in arid and semi-arid regions is the date palm tree (Phoenix
dactylifera L., family Arecaceae). As well, the date palm possesses a great position in the
spirits and minds of the societies of the Arab counties, in particular, the Middle East, and
north African regions. Additionally, it is abundant in several minerals and health enhancing
materials [1]. Along with the fruit palm tree leaves which applied as animal fodder once green
and as attractive objects after dry. Date fruits contains many vitamins such as: C, B1 and B2
[2]. Moreover, dates are healthy food with antioxidant, anticancer, and antiviral and activities

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[3, 4]. Further, dates contain substantial quantities of K, Na, Ca, Mg, P, Zn, Fe, and Cu [5].
However, the transition metals and metalloids like Cr, Ni, Be, Cd, Pb, and Pb are considered
as human carcinogens at extreme exposure [2].
Generally, heavy metals have been described to have both positive and negative characters to
human health because the body activities require them in certain levels. If these levels exceed,
the effects become negative. Certain metals like mercury, cadmium, and lead are major food
supply pollutants and it is considered the most crucial trouble to our environment. Others like
zinc, iron, and copper are necessary for biological activities in the human body. In general,
nearly all heavy metals have long biological half-lives and can be accumulated in cells and
tissues causing undesirable side effects [6]. Certain heavy metals are essential for plants
growth such as Zn, Fe, Co, Mn, Ni, and Cu and they play significant function in plant
metabolism. However, at elevated levels, they turn out to be toxic. In contrast, other heavy
metals such as Cd, `Pb, Hg, and as have been denoted with high toxicity for plants (even at
low levels) [7].
The growing heavy metals contamination in fruits and vegetables is due to the impact of
pesticides, fertilizers, and various industrial activities that pollute the air and soil [8]. Various
plants varieties have high capability to absorb heavy metals from the soil like
Mesembryanthemum absorbs 3% - 0.5% of the zinc and lead [9]. The plant's ability for heavy
metals accumulation in tissues depends on the plant size, growth speed, and the productivity
of biomass because they store them in different interweave. Therefore, the trees are the most
suitable for this critical process, since several trees have the ability to adapt and grow in
contaminated soils [10].
The evaluation of heavy metals in various kinds of food, biological, and environmental
samples has gained considerable interest due to various reasons with the most significant one
being the nutritional and toxic influences of these metals or their compounds [11]. Several
techniques of metal analysis were utilized in these determinations with the majority being
atomic absorption and atomic emission spectrometry [12]. The subsequent techniques have
been described for studies concerning with atomic absorption techniques: Flame Atomic
Absorption Spectrometry (F-AAS) [13–16], Electrothermal (or Graphite) Atomic Absorption
Spectrometry (ET-AAS) [17-19], Hydride Generated Atomic Absorption Spectrometry (HG-
AAS) [20], and Cold Vapour Atomic Absorption Spectrometry (CV-AAS). Likewise,
researches applying methods in relation to atomic emission techniques have also been
described. To these methods belong the following techniques: Inductively Coupled Plasma-
Optical Emission Spectrometry (ICP-OES) and Inductively Coupled Plasma- Mass
Spectrometry (ICP-MS) [21]. Beside these other uncommon metal analysis techniques like
spectrophotometric analysis, X-Ray Fluorescence (XRF), and Near IR Spectroscopy have
been applied [22, 23].
The objectives of the present research were to evaluate heavy metals in various date cultivars
and evaluation of their daily intake assessment from eating of dates. The health threats of
heavy metals to human beings are similarly described.

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2. Experimantal details
2.1. Sample Collection and Preparation
Five widespread Libyan dates varieties were chosen from Misurata city and gathered during
the harvest season (October 2020), which were: al-Tabouni (TAB), al-Bakrari (BAK), al-
Aami (AAM), al-Hamouri (HAM), and al-daqla (DAQ). Of each variety, about 2 kg was
gathered, sorted, affected fruits excluded, and the fleshy part from the cores separated, and in
the freezer kept. Next, the samples were initial oven-dried at 105oC for 24h. The dried
samples were then ground manually in a grinder for later use.
Moisture (%) was evaluated by drying a 5.0 g sample at 105°C to constant weight. Ash
content (%) was carried out on a 5.0 g sample after combustion in a muffle furnace at 550°C
for 2 h. The moisture content was calculated using the formula:
   
 (1)
Where: M1 and M2 stand for the mass before and after drying respectively.
The date sample is weighed before and after ashing (at 550oC for 2 hrs.) to determine the ash
percent. The ash content was be expressed on wet basis by the equation:
  
  (2)
Where: MASH refers to the mass of the ashed sample, and Msample refers to the original mass of
the wet samples.
2.2. Digestion Method
Digestion of the date samples was performed by adopting the wet method of Hseu [24] with
little modifications. 1.00 g of the sample was placed in a 250 mL glass beaker and 10 mL of
concentrated nitric acid was added. The samples were heated for 45 min at 90oC; later, the
temperature was increased to 150oC at which the samples were boiled for at least 2–3 h until a
clear solution was obtained. hydrogen peroxide was added to the sample (5 mL was added at
least three times) and digestion continued until the volume was reduced to about 1 mL. The
interior walls of the beaker were washed down with a little double distilled water and the
beaker was swirled throughout the digestion to keep the wall clean and prevent the loss of the
samples. After cooling, 5 mL of 1% HNO3 was added to the sample. Then, the solution was
filtered using Whatman No. 42 filter paper. The filtrate was then transferred to a 25 mL
volumetric flask and volume was made up using double distilled water.
2.3. Flame Atomic Absorption Analysis
Analysis for the heavy metals of interest was performed using atomic absorption spectrometry
technique (AA-7000 Hitachi Atomic Absorption spectrometer) with Deuterium lamp (D2-
lamp) background correction and hollow cathode lamps. Air–acetylene flame was used for
determination of all the elements. Measurements were made using standard hollow cathode
lamps for Pb, Cd, Zn, Cu, Mg, and Fe. Sodium, potassium, and calcium analysis was
conducted by PFP7 JENWAY Flame Photometer.
2.4. Chemicals and reagents
All the chemical reagents were of analytical grade. Standards. Standard solutions of the heavy
metals, namely, sodium (Na), potassium (K), calcium (Ca), magnesium (Mg), lead (Pb),
cadmium (Cd), copper (Cu), iron (Fe), and zinc (Zn), were provided by Merck (Darmstadt,
Germany). The standards were made from the individual 1000 mg/L standards (Merck)

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provided in 0.1N HNO3. A series of working standard solutions were prepared from these
standard stock solutions. Glassware was properly cleaned, and reagents used were of
analytical grades. Double distilled water was used throughout the study. Reagent blank
determinations were utilized to operate corrections to the instrument readings.
3. Results and discussion
3.1. Moisture and ash contents
The moisture and ash contents (%) are presented in Table 2 and illustrated in Figure 1.
Moisture levels for the five samples were ranged from 30-48%, with the highest percentage
being in the HAM cultivar (48%) and the lowest in the DAQ cultivar (30%). These results
were close to the study of (Hasanaoui et al., 2010) [25], where it was 31.9%, and the study of
(Sahari et al., 2007) [26], which showed a moisture content of 29.35%. Moreover, the results
of the current study were differed with the Ashraf and Hamidi-Esfahani study [27], where
their results showed that the average moisture were between 5-20%, as well as the (Taain et
al., 2013) study [28], in which the moisture content was 26.54%.
The ash contents for the five studied samples were very close. The DAQ cultivar had the
highest content with 1.52%, followed by TAB 1.16%, then by BAK and HAM with 1.14%
and 0.94, respectively, and finally the lowest was in AAM with 0.69%. Those obtained levels
were close to most previous studies, such as the study of (Besbes et al., 2004) [29] which
were 1.12-1.15%, the study of (Assirey., 2015) [30] where the levels ranged from 1.68 to
3.95%, and also (Hasanaoui et al., 2010) [25] study, since the ash contents ranged from 1.88
to 3.45%.
Table 1. Moisture and ash contents in the studied date samples
TAB
BAK
AAM
HAM
DAQ
% Moisture
40.0±2.0
39.0±1.9
36.0±1.8
48.0±2.5
30.0±1.3
% Ash
1.16±0.06
1.14±0.07
0.69±0.03
0.94±0.07
1.52±0.05
Figure 1. Moisture and ash contents in the studied date samples
0
10
20
30
40
50
60
TAB BAK AAM HAM DAQ
%
%Moisture
%Ash

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3.2. Metal Contents
The present research describes the major and minor (heavy) metals content in selected date
varieties available in the Misurata area of Libya. These metals were: Na, K, Ca, Mg, Zn, Fe,
Cu, Pb, and Cd. The detected mean concentrations of major and heavy metals found in the
studied samples are summarized in Tables 2 and 3. The metal concentrations determined were
based on the dry weight of sample.
Table 2. Major metals contents (mg/kg) in the studied date samples
TAB
BAK
AAM
HAM
DAQ
Na
38.0±1.9
17.0±0.8
31.0±1.4
69.0±3.1
19.1±1.0
K
2703.0±135.2
3075.1±150.8
3209.0±161.2
2146.1±104.3
3393.0±165.7
Ca
64.0±3.2
47.0±2.2
54.0±2.5
52.2±2.1
24.0±0.9
Mg
69.0±3.5
115.3±5.2
167.1±7.4
75.0±3.1
91.0±4.7
Table 3. Heavy metals contents (mg/kg) in the studied date samples
TAB
BAK
AAM
HAM
DAQ
Fe
127.9±6.1
9.4±0.5
8.4±0.3
28.0±1.6
10.7±0.5
Zn
12.2±0.6
12.0±0.6
7.4±0.4
13.6±0.7
8.0±0.4
Cu
3.9±0.2
3.8±0.2
3.3±0.1
5.5±0.2
0.54±0.03
Cd
0.21±0.01
0.44±0.02
0.22±0.03
0.14±0.04
1.02±0.05
Pb
UN
0.32±0.02
UN
UN
0.94±0.05
UN: under instrument detection limits
3.2.1. Potassium contents
Figure 2 displays the level of potassium in date samples. It is noted that the highest
concentration was in DAQ cultivar reaching 3393.0 mg/kg and the lowest value was in HAM
cultivar where were reached 2146.1 mg/kg. The potassium concentration is high denoting that
dates is a rich source for K. The elevated levels of K are attributed to the use of fertilizers
containing potassium [31]. Potassium is the most widespread cation in the intracellular fluid.
It is contained mostly inside the cells. It controls the osmotic pressure inside the cell, is
concerned in cell membrane transport and moreover in the initiation of a number of
respiratory and glycolytic enzymes [32]. Potassium levels were here found to be higher when
compared with similar samples in other countries, such as: Oribi (0.035 mg/kg) [33], Parvin
(460-680 mg/kg) [34], and Khan et al. (403-632 mg/kg) [35].

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Figure 2. Potassium contents in the studied date samples
3.2.2. Magnesium contents
Magnesium is a main constituent and play as an activator of many enzymes, especially those
related with the a of energy abounding phosphate compounds. Also, it acts a stabilizer of
plasma membranes, intracellular membranes, and nucleic acids. Magnesium lack causes
critical complaints due to its indispensable role in body metabolism [32]. The results showed
that the levels of Mg in all cultivars (Figure 3 and Table 2) ranged between 69.0 mg/kg in
TAB and 167.1 mg/kg in AAM. The lower level of Mg is within the range reported from
Sahari (18.4-79.4 mg/kg) [26]. However, the reported results in this study are higher that the
values reported for Parvin (48-53 mg/kg) [34] and Periyasamy and Padmanayaki (1.0 mg/kg)
[36] and lower than those of Mohamed 9925-2800 mg/kg) [37].
Figure 3. Magnesium contents in the studied date samples
0
500
1000
1500
2000
2500
3000
3500
4000
TAB AAM BAK HAM DAQ
mg/kg
0
20
40
60
80
100
120
140
160
180
TAB AAM BAK HAM DAQ
mg/kg

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3.2.3. Sodium contents
Sodium exhibit mainly as an extracellular ingredient and supports the osmotic pressure of the
extracellular fluid. Furthermore, it motivates some enzymes, such as amylase. From a
nutritional opinion, only the extreme intake of sodium is of importance due to it may lead to
hypertension [32]. Figure 4 illustrates the mean concentration of sodium in analyzed date
cultivars. Among the determined results, sodium depicted highest concentration (69.0 mg/kg)
in HAM cultivar followed by TAB (38.0 mg/kg) and minimum (17.0 mg/kg) in AAM
cultivar. The sodium contents were less than a pervious data reported by Attiya et. al. (15-405
mg/kg) [38]. On the other hand, the sodium concentrations were higher than reported by Oribi
(0.0661 mg/kg) [33] and Parvin (1-6 mg/kg) [34].
Figure4. Sodium contents in the studied date samples
3.2.4. Calcium contents
Figure 5 displays calcium contents of studied dates as determined by Flame Photometer. The
amount of Ca present in TAB is the highest among the samples (64.0 mg/kg). However, BAK
and HAM exhibited non-significant differences regarding calcium levels (54.0 and 52.2
mg/kg). Calcium concentrations in the present study are comparable with previous findings
for dates from Parvin (51-60 mg/kg) [34], Sahari (23.0-73.9 mg/kg) [26], and Khan (41.3-47.8
mg/kg) [35]. In the previous results [37, 38], Ca contents (3549- 4326 and 1413- 4340 mg/kg,
respectively) were very high compared to the results of the present study. The dates contain
suitable concentrations of calcium which is important for metabolism in human cells and also
essential for healthy bone development and for energy metabolism [30].
0
10
20
30
40
50
60
70
80
TAB AAM BAK HAM DAQ
mg/kg
×200
×200

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Figure5. Calcium contents in the studied date samples
3.2.5. Iron contents
Table 3 and Figure 6 show the average iron levels of date flesh from the five cultivars. A
considerable variation was observed with regard to Fe concentrations in the studied date
samples where the concentrations were found mostly higher in TAB (127.9 mg/kg) cultivar
than in the other cultivars (8.4-28.0 mg/kg). These values documented in this study is greater
than the results reached by Attiya (0.63-1.96 mg/kg) [38] and Oribi (0.03) [33] for dates from
both Libya and Iraq, respectively. Most of iron is exist mostly in both the hemoglobin (blood)
and myoglobin (muscle tissue) pigments. It is also present in several enzymes, such as:
hydroxylases, peroxidase, catalase, and flavine enzymes, consequently it is an essential
constituent of the daily diet [32].
Figure 6. Iron contents in the studied date samples
3.2.6. Zinc contents
Concentrations (mg/kg) of Zn in dry weight are shown in Figure 7 for 5 investigated date
samples. The highest concentration was reported for HAM with an average of 12.13 mg/kg,
whereas the lowest concentration was in AAM with a concentration of 5.8 mg/kg. Herein, we
0
10
20
30
40
50
60
70
TAB AAM BAK HAM DAQ
mg/kg
0
20
40
60
80
100
120
140
TAB AAM BAK HAM DAQ
mg/kg
a2)
b2)

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report higher concentrations compared to those of previous studies (0.07-1.78 mg/kg) [37, 39,
40]. However, this study is consistent with the findings of another previous study of Attiya
(9.3 mg/kg) [38]. Zinc metal constituents a number of enzymes like, glutamate
dehydrogenase, lactate dehydrogenase, alcohol dehydrogenase, malate dehydrogenase,
carboxypeptidases A and B, and carbonic anhydrase). Zinc can activate other enzymes, such
as, lecithinase, dipeptidases, alkaline phosphatase, and enolase [32].
Figure7. Zinc contents in the studied date samples
3.2.7. Copper contents
As shown in Figure 8, copper contents of the date samples ranged from 3.1 to 5.3 mg/kg.
HAM had the highest Cu content and AAM the lowest, with no significant difference between
TAB, AAM, and BAK cultivars. The results are higher than those reported previously by
Brima (0.10 mg/kg) [39], Takai (0.08-0.28 mg/kg) [40], and Attiya (0.11-0.12 mg/kg) [38].
Copper is an important metal for plants. Cu performs significant functions in photosynthetic
and respiratory electron transport chains, cell wall metabolism, oxidative stress protection, in
ethylene sensing, and biogenesis of molybdenum cofactor. Therefore, a lack in the copper
source may change essential operations in plant metabolism [41].
0
2
4
6
8
10
12
14
TAB AAM BAK HAM DAQ
mg/kg

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Figure 8. Copper contents in the studied date samples
3.2.8. Cadmium contents
The recorded results are shown in Figure 9 denote that the cadmium concentrations in TAB,
AAM and HAM cultivars were under the instrument detection limits, while BAK and DAQ
cultivars had cadmium contents ranging from 0.58 to 0.13 mg/kg, respectively. Cadmium can
cause kidney and lungs diseases, and also can result in skeleton problems as it is correlated
with cancerous hazard as compared with lead which is non-cancer risk issue [42]. The
detected Cd levels are due to various environmental reasons such as fertilizers applications to
soils, industrial emissions, mining, metallurgical operations, and non-biodegradation property
of metal [43].
Figure 9. Cadmium contents in the studied date samples
3.2.9. Lead contents
The results for lead, as shown in Figure 10, indicated the presence of Pb only in DAQ and BAK
cultivars since their concentrations ranged from 0.1 to 0.64 mg/kg. These results are supported by the
work of Mohamed [37] and also by Aldjain [1] who reported high level of Pb (0.96 mg/kg) released in
the environment. Lead is commonly inserted to the environment by aerial deposition on accessible
0
1
2
3
4
5
6
TAB AAM BAK HAM DAQ
mg/kg
0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
TAB AAM BAK HAM DAQ
mg/kg

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surfaces involving soil and plants parts. The increase of lead levels may be assigned to several reasons
while automobile influence to a greater extent subsequently by the usage of lead-based pesticides in
crop shield. The lead deposition on edible tissues of harvests similarly depends upon air pollution, air
dust, distance from the roads side in addition to traffic loads and extent of contact of products along
roadside for selling [42].
Figure 10. Lead contents in the studied date samples
Conclusion
The present study has expressed findings that are needed for future studies to describe the
mineral content of some widespread date cultivars in Libya. The results display those dates
have a high moisture content of (30–48%) and low ash levels (0.94–1.52%). The predominant
macro mineral was potassium followed by magnesium while the lowest was sodium. For the
essential heavy metals, iron had the highest concentration, followed by zinc, and the lowest
was copper. These results suggested that dates are a good source of essential elements and can
play a major task in human nutrition and health. Finally, DAQ and BAK cultivars contained
considerable amounts of Pb and Cd and in the other cultivars they were not detected. This
suggested that dates must be examined for HMs in order to avoid toxicity in humans.
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